Production of sealing and bottle-closing wax.



NITED STATES PATENT OFFICE.

WOLDEMAR ELLRAM, OF SIMFEROPOL, RUSSIA.

PRODUCTION OF SEALING AND BOTTLE-CLOSING WAX.

SPECIFICATION formingpart of Letters Patent No. 666,046, dated January15, 1901.

Application filed J ly 10, 1899. Serial No. 723,393. (No specimens.)

To all whom it may concern.-

Be it known that I, WOLDEMAR ELLRAM, a

- subject of the Emperor of Russia, and a resifor which such hasheretofore been used.

The sealing-wax hitherto manufactured, although practically waterproof,is not proof against the action of alcohols and alcoholic liquids. It ismore or less readily dissolved thereby, becomes soft and drops off,while the contents of the vessel sealed are often contaminated by thedissolved sealing-wax. On the other hand, sealing-wax as hithertomanufactured is too sensitive to climatic influences and temperaturevariations. At low temperatures it becomes brittle and is liable tocrack and peel ofi, and at higher temperatures it softens verymaterially.

This invention has for its object the manufacture of a sealing-wax freefrom the disadvantages referred tonamely, a sealing-Wax insoluble inalcohols generally, (ethyl and methyl), absolutely waterproof, andindifferent to the most varied climatic temperature variations. This Iattain by substituting for the resins hitherto employed, and which aresoluble in alcohol, their salts of the alkaline earths or earths andheavy metals which are insoluble in water, alcohol, or alcoholicliquids, as the resinates of calcium, magnesium, aluminium, iron, zinc,lead, and manganese. Experiments have shown that the resinic acids,especially abietic acid, which are insoluble in alcohol, are not onlynon-hygroscopic and have a comparatively high melting-point, but areparticularly well adapted as substitutes for the resinshitherto used inthe manufacture of sealing-wax, in that, irrespective of theirindiiference to the action of alcohols, they are also indifferent tomoisture and all climatic temperature variations. On the other hand,sealing-wax made of these resinates has the further advantage over thesealing-wax now in use in that it requires a much higher temperature tomelt it and does not therefore melt and drop off the stick when barelyignited or even before being ignited, as is the case with thesealing-wax now in use. In carrying out my invention I preferably usewhat is known as American or French resin or colophony, a transparentproduct free from water, the residue of the distillation of turpentineobtained from the pinus, abies, or larix, because it is an almost pureabietic acid. If, for instance, pulverized hydrate of lime (or calciumoxid) is added to melted colophony, foaming and evaporation of water inthe form of steam ensues under formation of the desired productnamely,calcium abietinate, which is insoluble in all alcohols generally. Ifoleic acidlis added to the aforesaid mixture, a reaction will take placein accordance with the following equation:

2(O H COOH)+Ca(OH),=

(C H GOO) Oa-i-2H O,

position: colophony, one hundred parts by.

weight; oleic acid, one hundred parts by weight; calcium hydrate, sevenparts by weight; solar oil, fourteen parts by weight; bariu m sulfate,one hundred parts, by weight.

Under the term solar oil I mean a hydrocarbon oil of a specific gravityof from 0.80 to 0.83 and a boiling-point of from 245 to 310 centigrade.

The compounding is or may be effected as follows: The colophonyorkindred resin is melted, preferably in a steam-jacketed vessel, and whenso melted the pulverized calcium hydrate and oleic acid are added. Theheating at a temperature of about 150 centigrade is continued until thewater separated has all been vaporized, when the reactions will havetaken place, after which the solar oil and the finely-pulverized bariumsulfate are added, and finally any suitable dyestuff or coloring-matter,these additions being of course effected under constant stirring of thesubstances, either by hand or mechau-' ically, so as to obtain anintimate admixture. In this compound the abietic acid and the oleic acidare not completely or fully combined with the baset'. e., the calcium inthis casethe sealing-wax being intended, for instance,for the sealin gof bottles containing liquids holding only about ninety per cent. ofethyl alcoholin solution. If, on the other hand, the sealing-wax is tobe used for sealing bottles holding pure ethyl or methyl alcohols, I add14.4 parts, by weight, more of calcium hydrate' a, 21.4 parts instead ofseven partsthe resulting sealing-wax also having a higher melting point.The sealingwax composed as described in the first example has amelting-point of about 115 centigrade; but by dispensing with the oleicacid the melting-point will be raised to about 140 centigrade. Of coursethe added constituents, as the barium sulfate and the solar oil, theformer as a filler, while the latter renders the sealing-wax moreductile, are both insoluble in alcohols and indifferent to climatictemperature variations.

Instead of barium sulfate chalk, magnesite,

zinc-white, infusorial earth, ocher, and the like may be used, andinstead of oleic acid.

certain oleates may be used which are likewise insoluble in alcohols-as,for instance, the palmitates and stearates-although less desirable onaccount of their high meltingpoint, so that by a proper choice andproportion of such substances the melting-point of the final product canbe varied from about 112 centigrade, or even lower, to about 160centigrade. I have found also that a slight excess of free abietic acidrenders the sealing-wax slightly soluble in alcohols; but this is'of noimportance in ageneral sense in view of the fact that the alcoholicliquids generally stored in sealed vessels do not contain sufficientalcohol to attack the sealing-wax, while this solubility can be readilyavoided by binding all of the free abietic acid in the manufacture ofsealing-wax for sealing bottles containing pure alcohols. This inventiontherefore lies, first, in the use of resinates, either Wholly insolublein alcohols or difficult of solution therein,preferably abietinatesindifferent to the action of alcohols, while by a proper compounding insuitable proportions the melting-point of the final product can bevaried within comparatively Wide limits.

I have hereinbefore stated that the resinate's of the metals of thealkaline earths, the earths, and heavy metals can be used, the reactionstaking place in accordance with the following equations, from which theproportions are deducible, the reaction in the case of calcium hydratehaving been given hereinbefore:

2(C H GOOH)+Zn(OH) Zn(C, H GOO) -|-2H O. 2(O I ,OOOH)+ZnO= Zn((3 H OOO)-{-H O.

Pb(O, H OO,O) -{-H O. 6(G H COOH)+A1 (OH) Al (G H COO) l-6H O.

Having thus described my invention, what I claim as new therein, anddesire to secure by Letters Patent, is-

1. The process, which consists in reacting upon a substance rich inabietic acid, as colophony and kindred resins, with an oxid or hydroxidof a metal of the alkaline earths or heavy metals to form an abietinateinsoluble or d-ifiicult of solution in alcohols, and mixing therewithasuitable filler and, if desired, coloring-matter, .both insoluble inalcohols, for the purpose set forth.

- 2. The process, which consists in reacting upon a substance rich inabietic acid, as colophony and kindred resins, with an oXid or hydroxidof the metals of the alkaline earths, or heavy metals, in the presenceof oleic acid, mixing therewitha suitable filler, and if desired,coloring-matter, both insoluble in alcohols, for the purpose setforth.

3. The process, which consists in reacting upon melted colophony orkindred resins with an oxid or hydroxid'of a metal of the alkalineearths, or heavy metals insoluble in alcohols, in the presence of oleicacid, mixing therewith a hydrocarbon insoluble in alcohols, a filler,and, if desired, coloring-matter, likewise insoluble in alcohols, forthe purposes set forth. 7

4:. The process, which consists in reacting upon melted colophony orkind red resins with calcium hydrate in the presence of oleic acid,

mixing therewith solar-oil or a kindred hydrocarbon insoluble inalcohol,bariu m sulfate or a kindred filler, and, if desired,coloringmatter insoluble in alcohols, substantially as set forth.

5. The herein-described sealing-wax, consisting essentially of anabietinate of a metal of the alkaline earths, or heavy metals, insolublein alcohols, a suitable filler and, if desired, a coloring-matter,substantially as set forth.

6. The herein-described sealing-wax, consisting essentially, of anabietinate and an In testimony that I claim the foregoing as oleate of ametal of the alkaline earths, or my invention I have signed my name inpres- IO heavy metals insoluble in alcohols, a hydroence of twosubscribing Witnesses.

carbon insoluble in alcohols, barium sulfate, or a kindred fillerinsoluble in alcohols, and, WOLDEMAR ELLRAM' if desired, acoloring-matter insoluble in alco- Witnesses: hols, substantially as andin about the propor- BOLESDANE HARODZIN, tions set forth. JULIUS S.KERUGEB.

